JP6961695B2 - Water-soluble unit dose article containing cyclic diamine - Google Patents

Description

The present invention relates to water-soluble unit dose articles containing cyclic diamines and methods of use thereof.

Water-soluble unit dose articles are preferred by consumers because of their convenience and ease of use. Consumers also like the fact that accidental leaks during the weighing operation are eliminated by eliminating the need to weigh the detergent input. Accidental weighing can be cumbersome and inconvenient.

However, the challenge for water-soluble unit dose articles is the possibility of premature rupture before use. Especially when the detergent composition is liquid, premature rupture can lead to leakage and cause troublesome conditions both in the storage container and during the weighing operation. In addition, leakage within the container can adversely affect adjacent unit dose articles, which can be cumbersome and inconvenient not only for the use of ruptured unit dose articles, but also for the use of adjacent unit dose articles. Means.

The viscosity of the liquid detergent composition can be increased to reduce the amount of leakage from the ruptured unit dose article. However, such an increase in viscosity requires the use of a rheology denaturant. Rheology denaturants do not provide the benefits of cleaning effects and only act to increase viscosity. This can be a problem for water-soluble unit dose articles where space for compounding the ingredients is limited. Therefore, the addition of the rheology denaturing agent can adversely affect the cleaning performance because the amount of the cleaning activator is reduced in order to create a space for blending the rheology denaturing agent.

Therefore, water-soluble unit-dose articles that provide excellent or even improved cleaning performance while minimizing the amount of liquid detergent leaking from prematurely ruptured unit-dose articles are sought in the art. Has been done. It is also desirable to minimize the effect of the liquid detergent composition on dissolution in water, preferably further improving dissolution, while minimizing the amount of liquid detergent leaking from prematurely ruptured unit dose articles. ing.

Surprisingly, it has been found that a water-soluble unit-dose article comprising a liquid detergent composition, wherein the liquid detergent composition comprises a cyclic diamine, solves the above technical problems. Was done.

A first aspect of the present invention is a water-soluble unit dose article comprising a water-soluble film and a liquid detergent composition, wherein the liquid detergent composition comprises a cyclic diamine, preferably a detergent composition. Containing 0.1 to 5% by weight, more preferably 0.1 to 2% by weight of the cyclic diamine, the cyclic diamine is the formula (I) of the formula (I):

式中、Ｒのうちの２つは、ＮＨ２、（Ｃ１〜Ｃ４）ＮＨ２、及びこれらの混合物からなる群から選択され、残りのＲは、独立して、Ｈ、１〜１０個の炭素原子を有する直鎖状又は分枝鎖状のアルキル又はアルケニルから選択され、液体洗剤組成物は、非石鹸アニオン性界面活性剤を含み、非石鹸アニオン性界面活性剤は、直鎖状アルキルベンゼンスルホネート、アルキルサルフェート、アルコキシル化アルキルサルフェート、又はこれらの混合物を含む、水溶性単位用量物品。

In the formula, two of R are selected from the group consisting of NH2, (C1 to C4) NH2, and mixtures thereof, and the remaining R independently contains H, 1 to 10 carbon atoms. Selected from linear or branched alkyl or alkenyl having, the liquid detergent composition comprises a non-soap anionic surfactant, the non-soap anionic surfactant is a linear alkylbenzene sulfonate, alkyl sulfate. , Alkylylated alkyl sulfates, or mixtures thereof, water-soluble unit dose articles.

A second aspect of the present invention is a step of adding a water-soluble unit dose article according to the present invention to sufficient water to dilute the liquid detergent composition at least 300 times to prepare a cleaning solution, and to prepare a cleaning solution, and to use the cleaning solution for the object to be cleaned. It is a cleaning method including a step of contacting with.

A third aspect of the invention is a packaged product comprising a resealable container and at least one water-soluble unit dose article according to the invention contained in the container.

A fourth aspect of the present invention provides the advantages of superior oil cleaning and reduction of liquid leakage from prematurely ruptured unit dose articles, improved dissolution of water soluble unit dose articles in water, or a combination thereof. , The use of cyclic diamine in a liquid detergent composition contained within a water-soluble unit dose article according to the present invention.

A schematic diagram of the basic configuration of the liquid detergent release test is shown.

Water-Soluble Unit-Dose Articles The present invention discloses a water-soluble unit-dose article comprising a water-soluble film and a liquid detergent composition. The water-soluble film and liquid detergent composition will be described in more detail below.

Water-soluble unit-dose articles include water-soluble films shaped such that the unit-dose articles contain at least one internal compartment surrounded by the water-soluble film. The unit dose article may include a first water-soluble film and a second water-soluble film that are sealed together to define an internal compartment. The water-soluble unit dose article is configured to prevent the detergent composition from leaking out of the compartment during storage. However, when the water-soluble unit dose article is added to water, the water-soluble film dissolves and the contents of the internal compartment are released into the cleaning solution.

It should be understood that compartment means a closed interior space within a unit dose article that holds the detergent composition. During production, the first water-soluble film may be shaped to include an opening compartment to which the detergent composition is added. Next, the first film is covered with the second water-soluble film in the direction of closing the opening of the compartment. The first and second films are then sealed together along the sealing area.

The unit dose article may include two or more compartments, further at least two compartments, or even at least three compartments. The compartments may be arranged in a superimposing orientation, i.e., so that one is located above the other. In such an orientation, the unit dose article comprises three films, top, center and bottom. Alternatively, the compartments may be located in a parallel orientation, i.e., one oriented adjacent to the other. The compartments may further be oriented in a "tire and rim" arrangement, i.e., the first compartment is located adjacent to the second compartment, but the first compartment at least partially the second compartment. However, it does not completely enclose the second compartment. Alternatively, one compartment may be completely enclosed within another compartment.

If the unit dose article comprises at least two compartments, one of the compartments may be smaller than the other compartments. If the unit dose article comprises at least three compartments, two of the compartments may be smaller than the third compartment, and preferably the smaller compartment may be overlaid on the larger compartment. The stacked compartments are preferably oriented in parallel.

In multi-compartment orientation, the detergent composition according to the invention may be contained within at least one of the compartments. For example, the detergent composition may be contained in only one compartment, or in two compartments, or even three compartments.

Each compartment may contain the same composition or different compositions. The different compositions may all have the same or different forms.

The water-soluble unit dose article may comprise at least two internal compartments, the liquid laundry detergent composition is contained within at least one of the compartments, preferably the unit dose article comprises at least three compartments and the detergent composition. Is included in at least one of the compartments.

Water-soluble film The film of the present invention is water-soluble or water-dispersible. The water-soluble film preferably contains polyvinyl alcohol or a copolymer thereof. Preferably, the water-soluble film is a combination of at least two different polyvinyl alcohol homopolymers, at least two different polyvinyl alcohol copolymers, at least one polyvinyl alcohol homopolymer and at least one polyvinyl alcohol copolymer, or a combination thereof. Including things.

Preferably, the water-soluble film has a thickness of 50 micrometers to 100 micrometers, preferably 70 micrometers to 90 micrometers, prior to transformation into a unit dose article.

Preferably, after using a glass filter with a maximum pore size of 20 μm, the water solubility of the film as measured by the methods described herein is at least 50%, preferably at least 75%, or even at least 95%.

To a pre-weighed 3 L beaker, 5 g ± 0.1 g of film material is added and 2 L ± 5 mL of distilled water is added. This is vigorously stirred at 600 rpm for 30 minutes at 30 ° C. with an electromagnetic stirrer (Labline model number 1250 or equivalent) and a 5 cm electromagnetic stirrer. The mixture is then filtered through a folded sintered glass filter for qualitative analysis with a pore size (up to 20 μm) as defined above. Water is dried from the recovered filtrate by any conventional method and the weight of the remaining material is determined (this is the dissolved or dispersed fraction). The solubility or dispersibility percentage can then be calculated.

The preferred film material is preferably a polymeric material. The film material can be obtained by, for example, cast molding, injection molding, extrusion molding or injection extrusion molding of a polymer material known in the art.

Preferred polymers, copolymers, or derivatives thereof suitable for use as pouch materials are polyvinyl alcohols, polyvinylpyrrolidones, polyalkylene oxides, acrylamides, acrylic acids, celluloses, cellulose ethers, cellulose esters, celluloseamides, polyvinylacetates, polys. It is selected from carboxylic acids and salts, polyamino acids or peptides, polyamides, polyacrylamides, maleic acid / acrylic acid copolymers, polysaccharides containing starch and gelatin, and natural rubbers such as xanthan and cara rubber. More preferred polymers are selected from polyacrylate and water soluble acrylate copolymers, methyl cellulose, sodium carboxymethyl cellulose, dextrin, ethyl cellulose, hydroxyethyl cellulose, hydroxypropyl methyl cellulose, maltodextrin, polymethacrylate, most preferably polyvinyl alcohol, polyvinyl alcohol copolymers and It is selected from hydroxypropyl methylcellulose (HPMC), as well as combinations thereof. Preferably, the concentration of the polymer in the pouch material, eg PVA polymer, is at least 60%. The polymer may have any weight average molecular weight, preferably from about 1000 to 1,000,000, more preferably from about 10,000 to 300,000, even more preferably from about 20,000 to. It is 150,000.

Preferably, the water soluble unit dose article comprises polyvinyl alcohol.

Also, a mixture of polymers may be used as the pouch material. This can be useful in controlling the mechanical and / or melting properties of the compartment or pouch, depending on its application and required needs. Suitable mixtures include, for example, mixtures in which the water solubility of one polymer is higher than that of another polymer and / or the mechanical strength of one polymer is higher than that of another polymer. Also, a mixture of polymers having different weight average molecular weights, such as PVA having a weight average molecular weight of about 10,000 to 40,000, preferably about 20,000 or a copolymer thereof, and about 100,000 to 300,000, preferably a copolymer thereof. A mixture with PVA having a weight average molecular weight of about 150,000 or a copolymer thereof is also suitable. Also, polymer blend compositions, such as hydrolyzable, water-soluble polymer blends (obtained by mixing polylactide and polyvinyl alcohol, typically about 1 to 35% by weight of polylactide, and about 65 to 65% by weight). Polymer blend compositions containing (such as polymer blends of polylactide and polyvinyl alcohol) containing 99% by weight of polyvinyl alcohol are also suitable herein.

Preferred for use herein are PVA polymers that have been hydrolyzed from about 60% to about 98%, preferably from about 80% to about 90%, with improved dissolution properties of the material.

A preferred film is one that exhibits good dissolution in cold water, i.e. unheated distilled water. Preferably, such films exhibit good dissolution at temperatures of 24 ° C, even more preferably 10 ° C. Good dissolution means that after the use of the above glass filter having a maximum pore size of 20 μm, the water solubility of the film measured by the method described herein is at least 50%, preferably at least 75%, or even at least. It means that it is 95%.

Preferred films are those supplied by Monosol.

The PVA resin is a first PVA polymer of about 30 to about 85% by weight or a first PVA polymer of about 45 to about 55% by weight of the total PVA resin content in the film described herein. Can include. For example, the PVA resin can contain about 50% by weight of each PVA polymer, the first PVA polymer has a viscosity of about 13 cP, and the second PVA polymer has a viscosity of about 23 cP (desorption at 20 ° C.). Measured as a 4% polymer solution in salt water).

Preferably the film comprises a formulation of at least two different polyvinyl alcohol homopolymers and / or copolymers.

Most preferably, the water soluble film comprises a formulation of at least two different polyvinyl alcohol homopolymers, particularly a formulation of at least two different polyvinyl alcohol homopolymers having different average molecular weights, in particular two different polyvinyl alcohols. _{When the absolute value of the difference in average viscosity | μ 2-} μ ₁ | of the first PVOH homopolymer and the second PVOH homopolymer in the homopolymer formulation is measured as a 4% polymer solution in desalted water. Formulations of two different polyvinyl alcohol homopolymers ranging from 5, 5 cP to about 15 cP, and both homopolymers have an average degree of hydrolysis of 85% to 95%, preferably 85% to 90%. include. The first homopolymer preferably has an average viscosity of 10 to 20 cP, preferably 10 to 15 cP, and the second homopolymer preferably has an average viscosity of 20 to 30 cP, preferably 20 to 25 cP. Most preferably, the two homopolymers are blended in a weight% ratio of 40/60 to 60/40.

Alternatively, the water-soluble film comprises a polymer blend containing at least one copolymer containing polyvinyl alcohol and an anion-modified monomeric unit. In particular, this polymer blend may contain polyvinyl alcohol homopolymers and copolymers containing polyvinyl alcohol and anion-modified monomeric units in a weight% ratio of 90/10 to 50/50. Alternatively, the polymer blend may contain two different copolymers containing polyvinyl alcohol and anion-modified monomeric units in a weight% ratio of 90/10 to 10/90.

Common types of anionic monomer units that can be used in PVOH copolymers are monocarboxylic acid vinyl monomers, their esters and anhydrides, dicarboxylic acid monomers with polymerizable double bonds, their esters and anhydrides, vinyl sulfonic acid monomers. , And the vinyl polymerization unit corresponding to any of the alkali metal salts described above. Examples of suitable anionic monomers include vinyl polymerization units corresponding to vinyl anionic monomers, which vinyl anionic monomers include vinylacetic acid, maleic acid, monoalkyl maleate, dialkyl maleate, monomethyl maleate. , Dimethyl maleate, maleic anhydride, fumaric acid, monoalkyl fumarate, dialkyl fumarate, monomethyl fumarate, dimethyl fumarate, fumarate anhydride, itaconic acid, monomethyl itacone, dimethyl itaconate, itaconic anhydride, vinyl sulfonic acid Acid, allyl sulfonic acid, ethylene sulfonic acid, 2-acrylamide-1-methylpropansulfonic acid, 2-acrylamide-2-methylpropanesulfonic acid, 2-methylacrylamide-2-methylpropanesulfonic acid, 2-sulfoethylacrylate, the alkali metal salts (e.g., sodium, potassium or other alkali metal salt), the esters (e.g., methyl, ethyl, or other C ₁ -C ₄ or C ₆ alkyl esters,), and these Combinations (eg, multiple types of anionic monomers, or equivalents of the same anionic monomer) can be mentioned. In one embodiment, the anionic monomer is an acrylamide methylpropanesulfonic acid (eg, 2-acrylamide-1-methylpropanesulfonic acid, 2-acrylamide-2-methylpropanesulfonic acid, 2-methylacrylamide-2-methylpropanesulfonic acid). It can be an acid), an alkali metal salt thereof (eg, a sodium salt), and one or more of these combinations. In one embodiment, the anionic monomer can be one or more of monomethyl maleate, an alkali metal salt thereof (eg, a sodium salt), and a combination thereof.

The level of incorporation of one or more anionic monomer units in the PVOH copolymer is not particularly limited. In some embodiments, one or more anionic monomeric units are present in the PVOH copolymer individually or in total in an amount ranging from about 2 mol% to about 10 mol% (eg, various). In the embodiment of, at least 2.0, 2.5, 3.0, 3.5 or 4.0 mol% and / or maximum about 3.0, 4.0, 4.5, 5.0, 6 0.0, 8.0 or 10 mol%).

Of course, different film materials and / or films of different thicknesses may be used to make the compartments of the invention. The advantage of choosing different films is that the resulting compartments can exhibit different solubility or release properties.

In addition, the film material of the present specification may contain one or more additive-containing components. For example, it may be beneficial to add plasticizers such as glycerol, ethylene glycol, diethylene glycol, propylene glycol, dipropylene glycol, sorbitol, and mixtures thereof. Other additives may include water and functional detergent additives, including surfactants delivered to wash water, such as organic polymer dispersants.

The film may be opaque, transparent or translucent. The film may include a printed area. The printed area is 10% to 80% of the film surface, or 10% to 80% of the film surface in contact with the interior space of the compartment, or% 10 to 80% of the film surface and 10% to 10% of the compartment surface. It may reach 80%.

The print area may extend to a continuous portion of the film, or a portion of the continuous portion, i.e. the narrower area of the print, the sum of which is the internal space of the film surface or compartment. Corresponds to 10% to 80% of the film surface in contact and / or both.

The print area may include inks, pigments, dyes, bluish agents, or mixtures thereof. The print area may be opaque, translucent, or transparent.

The print area may include a single color, or may include a plurality of colors, or even three colors. The print area may include white, black, blue, red, or a mixture thereof. The print may be present as a layer on the surface of the film or may at least partially penetrate into the film. The film includes a first side and a second side. The print area may be on one side of the film or on both sides of the film. Alternatively, the print area may be included at least partially within the film body.

The print area may contain ink, which contains pigments. The ink for printing on the film is preferably of the desired dispersion grade in water. The ink may be any color including white, red, and black. The ink may be a water-based ink containing 10% to 80%, or 20% to 60%, or 25% to 45% water by weight. The ink may contain 20% to 90%, or 40% to 80%, or 50% to 75% solids by weight.

The viscosity of the ink may be 1-600 cPs, or 50-350 cPs, or 100-300 cPs, or 150-250 cPs, measured at a shear rate of 1000 s- ^{1 at 20 ° C.} This measurement result can be obtained by the cone plate shape with the TA Instruments AR-550 rheometer.

The print area can be obtained using standard techniques such as flexographic printing or inkjet printing. Preferably, the print area is obtained via flexographic printing, in which case the film is printed and then molded into the shape of the opening compartment. Next, the detergent composition is filled in this compartment, and a second film is placed above the compartment and sealed into the first film. The print area may be on one side or both sides of the film.

Alternatively, inks or pigments may be added during the production of the film so that all or at least a portion of the film is colored.

The film may contain an aversive agent, such as a bitterant. Suitable bitterants include, but are not limited to, naringin, saccharose octaacetate, quinine hydrochloride, denatonium benzoate, or mixtures thereof. Any suitable concentration of aversive agent may be used on the film. Suitable concentrations include, but are not limited to, 1 to 5000 ppm, or even 100 to 2500 ppm, or even 250 to 2000 ppm.

Liquid Detergent Compositions Water-soluble unit dose articles include liquid detergent compositions. The term "liquid detergent composition" means any detergent composition that includes a liquid that can wet and process an article or surface, such as washing clothes in a household washing machine, and is limited. Examples thereof include liquids, gels, pastes, and dispersions. The liquid composition may contain a solid or a gas in an appropriately divided form, but the liquid composition excludes an overall non-fluid form such as tablets or granules.

The liquid detergent composition is preferably selected from laundry detergent compositions, automatic dishwashing compositions, hard surface cleaners, and mixtures thereof.

The liquid detergent composition may be used as a fully formulated consumer product or may be added to one or more additional ingredients to make a fully formulated consumer product. ..

The liquid detergent composition may be a "pretreatment" composition that is added to the fabric, preferably a stain on the fabric, prior to adding the fabric to the cleaning solution.

The liquid detergent composition may be used in a fabric hand-washing operation or in a fabric washing operation in an automatic washing machine.

The liquid detergent composition is of formula (I):

の環状ジアミンを含み、式中、Ｒのうちの２つは、ＮＨ２、（Ｃ１〜Ｃ４）ＮＨ２、及びこれらの混合物からなる群から選択され、残りのＲは、独立して、Ｈ、１〜１０個の炭素原子を有する直鎖状又は分枝鎖状のアルキル又はアルケニルから選択される。

In the formula, two of the R's are selected from the group consisting of NH2, (C1-C4) NH2, and mixtures thereof, and the remaining Rs are independently H, 1- It is selected from linear or branched alkyl or alkenyl having 10 carbon atoms.

The term "cyclic diamine" is used herein to include a single wash amine and mixtures thereof. The amine can be subjected to protonation depending on the pH of the wash medium in which it is used.

The amine of formula (I) is a cyclic amine having two primary amine functional groups. The primary amine can be present at any position in the ring, but from the viewpoint of oil cleaning, it has been found that better performance can be obtained when the primary amine is present at the 1st and 3rd positions. It has also been found that amines, one of which is -CH3 and the rest is H, are advantageous from the viewpoint of oil and fat cleaning.

Preferably, the "remaining R" of formula I is selected from H, CH3, and mixtures thereof.

With respect to Formula I, the two Rs selected from the group consisting of NH2, (C1-C4) NH2, and mixtures thereof are preferably at positions R1 and R3 of Formula I.

Cyclic diamine

及びこれらの混合物からなる群から選択され得る。

And can be selected from the group consisting of mixtures thereof.

The cyclic diamine is selected from the group consisting of 1,3-bis (methylamine) -cyclohexane, 2-methylcyclohexane-1,3-diamine, 4-methylcyclohexane-1,3-diamine, and mixtures thereof.

The liquid detergent composition may contain 0.1% to 5% by weight, preferably 0.1% to 2% by weight of cyclic diamine of the liquid detergent composition.

The liquid detergent composition comprises a non-soap anionic surfactant. The liquid detergent composition may contain a surfactant and is preferably selected from anionic surfactants, nonionic surfactants, cationic surfactants, bipolar ion surfactants and amphoteric surfactants. .. Preferably, the surfactant is selected from anionic surfactants, nonionic surfactants, amphoteric surfactants, and mixtures thereof.

The anionic surfactant may include soap. Non-soap anionic surfactants include linear alkylbenzene sulfonates, alkyl sulphates, alkoxylated alkyl sulphates, or mixtures thereof. Preferably, when the non-soap anionic surfactant comprises a linear alkylbenzene sulfonate and an alkoxylated alkyl sulphate, the weight ratio of the linear alkyl benzene sulfonate to the alkoxylated alkyl sulphate is preferably 2: 1 to 1: 8. Is 1: 1 to 1: 5, most preferably 1: 1.25 to 1: 4.

The liquid laundry detergent composition is 5% to 45% by weight, preferably 10% to 40% by weight, more preferably 15% to 35% by weight, and most preferably 20% to 30% by weight of the liquid detergent composition. May contain% non-soap anionic surfactant.

The liquid laundry detergent composition comprises 5% to 35% by weight, preferably 5% to 20% by weight, more preferably 5% to 15% by weight of a non-soap anionic surfactant of the liquid laundry detergent composition. May include.

The amphoteric surfactant may comprise an amine oxide, more preferably the amine oxide is selected from C _12-14 dimethylamine oxide or C _12-14 amidpropyl dimethylamine oxide, preferably C _12-14 dimethylamine oxide. , Most preferably _{selected from linear C 12-14} dimethylamine oxides. When an amphoteric surfactant, preferably an amine oxide surfactant, is included, the liquid laundry detergent composition is 0.01% to 20% by weight, preferably 0.2% to 15% by weight, of the liquid detergent composition. More preferably 0.5% by weight to 10% by weight, most preferably 1% by weight to 5% by weight of an amphoteric surfactant, preferably an amine oxide surfactant is contained.

The liquid detergent composition may contain a nonionic surfactant, preferably the nonionic surfactant is an aliphatic alcohol alkoxylate, an oxo synthetic aliphatic alcohol alkoxylate, a gelber alcohol alkoxylate, an alkylphenol alcohol alkoxylate. , Or a mixture of these. Preferably, the weight ratio of the non-soap anionic surfactant to the nonionic surfactant is 1: 1 to 20: 1, preferably 1.3: 1 to 15: 1, more preferably 1.5: It is 1 to 10: 1.

The liquid laundry detergent composition is a nonionic surfactant of 1% to 25% by weight, preferably 1.5% by weight to 20% by weight, most preferably 2% by weight to 15% by weight of the liquid laundry detergent composition. May include.

The liquid detergent composition is 1% by weight to 25% by weight, preferably 1.5% by weight to 20% by weight, more preferably 1% by weight to 25% by weight, preferably 1.5% by weight to the liquid detergent composition. It may contain 20% by weight, most preferably 2% to 15% by weight of soap.

The liquid laundry detergent composition may include a cleaning polymer or a care polymer, preferably the cleaning polymer or the care polymer is ethoxylated polyethyleneimine, alkoxylated polyalkylphenol, amphoteric graft copolymer, polyester terephthalate, hydroxyethyl cellol. , Carboxymethyl cellulose, or mixtures thereof.

Liquid detergent compositions include hue dyes, polymers, builders, dye transfer inhibitors, dispersants, enzymes, enzyme stabilizers, catalyst materials, bleaching agents, bleach activators, polymer dispersants, anti-redeposition agents, foam inhibitors. , Aesthetic dyes, bleaching agents, fragrances, fragrance delivery systems, structuring agents, hydrotropes, processing aids, pigments, and auxiliary ingredients selected from mixtures thereof.

Preferably, the liquid laundry detergent composition is non-Newtonian. Although not bound by theory, non-Newtonian fluids have different properties than Newtonian fluids, and more specifically, the viscosity of non-Newtonian fluids is independent of shear rate and Newtonian fluids. Has a constant viscosity regardless of the applied shear rate.

The liquid detergent composition can have a viscosity of at least 2 Pa · s at a shear rate of ^{0.5 s -1} when measured using TA Rheometer AR2000 at 25 ° C., preferably the liquid detergent composition When measured using TA Rheometer AR2000 at 25 ° C., at ^{a shear rate of 0.5 s-1} , 2 Pa · s to 35 Pa · s, preferably 2.5 Pa · s to 30 Pa · as, more preferably 3 Pa · s. It has a viscosity of ~ 25 Pa · s, even more preferably 5 Pa · s to 20 Pa · s, most preferably 10 Pa · s to 16 Pa · s.

The liquid detergent composition may include a non-aqueous solvent. Non-aqueous solvents include polyethylene glycol (PEG) polymers with molecular weights of 300 and 600, dipropylene glycol (DPG), nbutoxypropoxypropanol (nBPP), 1,2-propanediol, 1,3-propanediol, glycerol, ethanol, etc. And can be selected from the group containing mixtures thereof, preferably the non-aqueous solvent comprises dipropylene glycol (DPG), n butoxypropoxypropanol (nBPP), 1,2-propanediol, glycerol, and mixtures thereof. Can be selected from the group.

Cleaning Method Further embodiments of the present invention include a step of adding a water-soluble unit dose article according to the present invention to sufficient water to dilute the liquid detergent composition at least 300 times to prepare a cleaning solution, and the object to be cleaned. It is a cleaning method including a step of contacting with a cleaning liquid.

Packaged Product A further aspect of the invention is a packaged product comprising a resealable container and at least one water-soluble unit dose article according to the invention contained in the container.

Those skilled in the art will recognize suitable storage containers. Preferably, the storage container is flexible, preferably resealable, baggage, rigid, preferably resealable, tabbed container or a mixture thereof, preferably book storage. The container is equipped with a pediatric safety lid. Those skilled in the art will recognize suitable pediatric safety lids.

The package can be made from any suitable material. Containers can be made from metal materials, aluminum, plastic materials, cardboard materials, laminates, cellulosic pulp materials, or mixtures thereof. The package can be made from a plastic material, preferably a polyolefin material. Packages can be made from polypropylene, polystyrene, polyethylene, polyethylene terephthalate, PVC or mixtures thereof, or more durable engineering plastics such as acrylonitrile butadiene styrene (ABS), polycarbonate, polyamide. The materials used to make the container may include other ingredients such as colorants, preservatives, plasticizers, UV stabilizers, oxygen, fragrances and moisture barrier recycled materials.

Use A further aspect of the invention is to provide the benefits of superior oil cleaning and reduction of liquid leakage from prematurely ruptured unit dose articles, improved dissolution of water soluble unit dose articles in water, or a combination thereof. The use of cyclic diamine in a liquid detergent composition contained within a water-soluble unit dose article according to the present invention.

The dimensions and values disclosed herein should not be understood as being strictly limited to the exact numbers listed. Rather, unless otherwise indicated, each such dimension shall mean both the stated value and the functionally equivalent range around that value. For example, the dimension disclosed as "40 mm" is intended to mean "about 40 mm".

The following detergent compositions were prepared using standard mixing techniques.

Ｂａｘｘｏｄｕｒ ＥＣＸ２１０：４−メチルシクロヘキサン−１，３−ジアミン及び２−メチルシクロヘキサン−１，３−ジアミンの環状ジアミン混合物、ＢＡＳＦから入手可能。

Baxxodur ECX210: A cyclic diamine mixture of 4-methylcyclohexane-1,3-diamine and 2-methylcyclohexane-1,3-diamine, available from BASF.

A single compartment water-soluble unit dose article with an installation area of 50 x 50 mm, a cavity depth of 20.79 mm, and a cavity volume of 34 mL was prepared by heat / vacuum forming and filled with the above composition. An M8630 water-soluble film commercially available from Monosol was used.

Reference unit dose articles containing reference detergent compositions were outside the scope of the present invention. Unit-dose articles containing the detergent composition of Example A Example A was within the scope of the present invention.

Early burst release test method:
The test method uses a Pinhole-inclusive unit dose using an Instron Universal Products (825 University Avenue., Norwood, MA 02062-2643) equipped with a load cell of up to 100 kN (kilonewton). A method for determining the sensitivity of a liquid detergent composition flowing out of an article under pressure will be described. In this method, a liquid flowing out of a unit dose article is measured by applying pressure to the unit dose article at a constant pressure (100 N) for a certain period of time (3 seconds) and measuring the weight of the unit dose article before and after pressurization. The total amount of the detergent composition is determined by weight.

The test is performed immediately 2 weeks after production of the unit dose article to allow time for the film / unit dose to remain constant after processing. The method is performed in an indoor environment of 40-50% relative humidity (RH) and 22-24 ° C. Unit-dose articles are equilibrated in the laboratory environment for 1 hour prior to testing. Immediately prior to the test, a 1 mm diameter needle is used to manually pinhole the underside of the sealing area of the unit dose article.

FIG. 1 shows a schematic diagram of the basic configuration of a liquid detergent release test. A reference unit dose article and a test unit dose article 510 are placed between two compression plates 520 and 530 of the instrument to measure the amount of liquid detergent released from the unit dose article containing pinholes. The side wall of the pinhole 511 of the unit dose article should not be covered with a plate so that the liquid detergent can be freely drained from the unit dose article. The unit dose article 510 is arranged such that the plane including the sealing flange region 540 is located horizontally and perpendicular to the direction of the force applied by the compression plate (x direction). For single compartment unit dose articles and side-by-side multi-compartment unit dose articles, a deformable film that allows detergent to be added through the cavity is brought into contact with the lower compression plate, and the sealed film is placed on the upper compression plate. To contact. For side-by-side multi-segment unit dose articles, all individual compartments, including the liquid detergent, are perforated directly below the encapsulation region, as described above. For superposition unit dose articles, the maximum volume portion is brought into contact with the lower compression plate to provide one hole. To pressurize, the rate of narrowing the distance between the plates 520 and 530 is set to 150 mm / min, and when the pressure of 100 N reaches the unit dose article, it is maintained for 3 seconds and then the pressure is released. Unit dose Weigh the article before and after pressurization. The differential weight (in grams) corresponds to the amount of detergent composition leaked from the unit dose article. Repeat 3 times for each test leg and report the average loss value of the detergent composition.

Dissolution test method for unit dose articles:
The dissolution test method for a unit-dose article aims to determine the dissolution time of the unit-dose article in water by measuring the conductivity over time. After production, the unit dose article is stored at 23 ° C., 50% RH for 2 weeks to equilibrate the detergent composition / film.

A 5 L glass beaker (17 cm in diameter) is filled with 3 L of desalinated water (19-21 ° C., conductivity <5 μS. Cm). Connect a 4-blade impeller (diameter 10 cm, model IKA R1345) to a mechanical stirrer (type: IKA Eurostar Power Control), set the stirring speed to 70 rpm, and set the upper part of the impeller blades to the 1000 mL scale of the beaker. Adjust the height so that it is located. The conductivity probe (type: Mettler Toledo Seven Excellence) and temperature probe are adjusted in height so that the bottom of the probe is located on the 2000 mL scale of the beaker.

The unit dose article is sufficient to hold the unit dose article in a fixed and reproducible position in aqueous solution, i.e., at 1/3 of the height of the outer water column when agitated. Place in a sized metal holder. The mesh size of the holder is chosen so that it does not substantially affect the flow of water and therefore does not affect the dissolution experiment. The unit dose article is arranged so that the sealing surface of the unit dose article is in a vertical position and thus is substantially orthogonal to the flow of water. When testing unit dose articles of similar size, reuse the same holder for different test legs to minimize data variability.

The conductivity and temperature of the aqueous solution are measured every 5 seconds for a total test time of 15 minutes, and the measurement begins as soon as the unit dose article is immersed in the aqueous solution and placed in its fixed position almost instantly. The individual conductivity measurements are normalized to the completion value (%) according to the following equation.

導電率（Ｔ）は、時点ｔで測定された導電率であり、最小導電率は、１回目、すなわち、水溶性パウチを浸漬したときの導電率測定点であり、最大導電率は、１５分後に測定された導電率である。

The conductivity (T) is the conductivity measured at time point t, the minimum conductivity is the first conductivity measurement point when the water-soluble pouch is immersed, and the maximum conductivity is 15 minutes. The conductivity measured later.

As a result, all the individual completion values (%) for each film are accumulated and the average of 3 repetitions is reported. The higher the accumulated completion value (%), the faster the water-soluble unit dose article dissolves.

result:
From the data in Table 2, the single variable addition of the cyclic diamine (Example A) according to the present invention causes pinholes when pressure is applied compared to the reference liquid which does not contain the cyclic diamine according to the present invention. It is clear that this leads to a reduction in the amount of liquid leaking from the water-soluble unit dose article provided.

Table 3 below shows that in the liquid composition containing the cyclic diamine according to the present invention, the dissolution profile was delayed even though the leakage from the pinhole-provided unit dose article was prolonged as described above. It shows that it does not occur. In fact, in the unit dose article according to the present invention (Example A), faster dissolution of the unit dose article was observed.

Claims (13)

A water-soluble unit dose article comprising a water-soluble film and a liquid detergent composition, wherein the liquid detergent composition comprises 0.1% to 5% by weight of cyclic diamine of the liquid detergent composition. , The cyclic diamine is selected from the group consisting of 2-methylcyclohexane-1,3-diamine, 4-methylcyclohexane-1,3-diamine, and mixtures thereof, and the liquid detergent composition is the liquid detergent composition. Containing 5% to 35% by weight of a non-soap anionic surfactant, said non-soap anionic surfactant comprises a linear alkylbenzene sulfonate, an alkyl sulphate, an alkoxylated alkyl sulphate, or a mixture thereof. , Water-soluble unit dose articles. The water-soluble unit dose article of claim 1, wherein the liquid detergent composition comprises soap. The water-soluble unit dose article of claim 1 or 2 , wherein the non-soap anionic surfactant comprises a linear alkylbenzene sulfonate and an alkoxylated alkyl sulfate. The water-soluble unit dose article according to any one of claims 1 to 3 , wherein the liquid detergent composition contains an amphoteric surfactant, and the amphoteric surfactant contains an amine oxide. The liquid detergent composition comprises a nonionic surfactant, wherein the nonionic surfactant is an aliphatic alcohol alkoxylate, an oxo synthetic aliphatic alcohol alkoxylate, a gelber alcohol alkoxylate, an alkylphenol alcohol alkoxylate, or an alkylphenol alcohol alkoxylate. The water-soluble unit dose article according to any one of claims 1 to 4 , which is selected from these mixtures. The water-soluble unit dose article according to claim 5 , wherein the weight ratio of the non-soap anionic surfactant to the nonionic surfactant is 1: 1 to 20: 1. The water-soluble unit dose article of claim 5 or 6 , wherein the liquid detergent composition comprises 1% to 25% by weight of the nonionic surfactant of the liquid detergent composition. The water-soluble unit dose article according to any one of claims 1 to 7 , wherein the liquid detergent composition is a laundry detergent composition. The water-soluble unit dose article according to any one of claims 1 to 8 , wherein the water-soluble film is a polymer water-soluble film. Any one of claims 1 to 9 , wherein the liquid detergent composition has a viscosity of at least 2 Pa · s at a shear rate of ^{0.5 s -1} when measured using TA Rheometer AR2000 at 25 ° C. A water-soluble unit dose article according to. A step of adding the water-soluble unit dose article according to any one of claims 1 to 10 to sufficient water to dilute the liquid detergent composition at least 300 times to prepare a cleaning liquid, and a step of preparing a cleaning liquid, and a process to be cleaned. A cleaning method comprising a step of contacting with the cleaning liquid. A packaged product comprising a resealable container and at least one water-soluble unit dose article according to any one of claims 1 to 10 contained within the container. Claims 1-10 to provide the advantages of superior oil and fat cleaning and reduced liquid leakage from prematurely ruptured water-soluble unit-dose articles, improved dissolution of water-soluble unit-dose articles in water, or a combination thereof. Use of a cyclic diamine in a liquid detergent composition contained in the water-soluble unit dose article according to any one of the above , wherein the cyclic diamine is 2-methylcyclohexane-1,3-diamine, 4-methylcyclohexane. Use, selected from the group consisting of -1,3-diamine, and mixtures thereof.

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